Resumo em Inglês:

2,4 - Dimethoxybenzoates of Mn(II), Co(II) and Cu(II) have been synthesized as hydrated or anyhydrous polycrystalline solids and characterized by elemental analysis, IR spectroscopy, magnetic studies and X-ray diffraction measurements. They possess the following colours: Mn(II) - white, Co(II) - pink and Cu(II) - blue. The carboxylate groups bind as monodentate, or a symmetrical bidentate bridging ligands and tridentate. The thermal stabilities were determined in air at 293-1173K. When heated the hydrated complexes dehydrate to from anhydous salts which are decomposed to the oxides of respective metals. The magnetic susceptibilites of the 2,4-dimethoxybenzoates were measured over the range 76-303 K and their magnetic moments were calculated. The results reveal the complexes of Mn(II), Co(II) to be high-spin complexes and that of Cu(II) to form dimer.

Resumo em Português:

O fracionamento cromatográfico da fase diclorometânica dos caules de Michelia champaca, forneceu quatro substâncias: álcool 4-O-beta-D-glicopiranosídeo sinapílico, aldeído 4-O-beta-D-glicopiranosídeo sinápico, siringaresinol e N-acetilnonaina. Extração ácido-base de uma nova porção do extrato bruto etanólico permitiu a identificação do alcalóide liriodenina. Os derivados fenilpropanoídicos e o alcalóide N-acetilnonaina estão sendo descritos pela primeira vez no gênero Michelia. O alcalóide liriodenina e a lignana siringaresinol apresentaram atividade antifúngica moderada.

Resumo em Inglês:

The fractionation of the dichlorometanic layer of dried stems of Michelia champaca afforded four substances: sinapyl 4-O-beta-D-glucopyranoside alcohol, sinapyl 4-O-beta-D-glucopyranoside aldehyde, syringaresinol and N-acetylnonaine. Part of the crude extract portion was submitted to acid-basic extraction allowed the identification of the alkaloid liriodenine. The two phenylpropanoids derivatives and the alkaloid N-acetylnonaine were been reported for the first time from Michelia genus. The alkaloid liriodenine and the lignan syringaresinol showed moderate antifungal activity.

Resumo em Inglês:

A novel heteronuclear 3d-4f compound having formula NdCu3L3·13H2O (where H3L = Schiff base derived from 5-bromosalicylaldehyde and glycylglycine and L³ = C11H8 N2O4Br) was obtained. It was characterized by elemental and thermal analyses and magnetic measurements. The Cu(II)-Nd(III) compound is stable up to 323 K. During dehydration process the water molecules are lost in two stages. The magnetic susceptibility data for this complex change with temperature according to the Curie-Weiss law with theta = -35 K. The magnetic moment values decrease from 5.00µB at 303 K to 4.38µB at 76 K.

Resumo em Português:

Um sistema de injeção em fluxo envolvendo a adição de amostra e reagente por zonas coalescentes sincronizadas é proposto para a determinação de cálcio em leites por FAAS. Um planejamento fatorial com ponto central auxiliou na seleção dos principais parâmetros experimentais, sendo as condições ótimas estabelecidas em: solução de lantânio 2,5% (m/v), vazão do transportador 8 mL min-1, comprimento da bobina de reação 20 cm e volume de amostra injetado 250 ìL. Quatro procedimentos de preparo de amostra foram avaliados: diluição em ácido nítrico diluído e em água, decomposição em forno de microondas empregando ácidos concentrados e diluídos. O sistema de análise por injeção em fluxo desenvolvido foi aplicado na determinação de cálcio em onze amostras de leite comerciais e em dois materiais de referência padrão diluídos em água. Teores similares de cálcio foram encontrados comparando-se os resultados obtidos pelo método proposto (diluição em água) com aqueles obtidos nos digeridos. As concentrações de cálcio determinadas nos dois materiais de referência padrão foram concordantes a um nível de 95% de confiança com seus valores certificados. Recuperações entre 93% a 116% foram obtidas. O desvio padrão relativo (n = 12) foi < 5,4% e a freqüência analítica equivalente a 150 medidas por hora, correspondendo a um consumo de 250 ìL de amostra e 6,25 mg de lantânio por determinação.

Resumo em Inglês:

A flow-injection system with sample and reagent addition by the synchronous merging zones approach for calcium determination in milk by flame AAS is proposed. Main parameters were optimized using a factorial design with central point. The optimum conditions were 2.5% (m/v) for La concentration, 8 mL min-1 for the carrier flow-rate, 20 cm for coiled reactor and 250 ìL for sample volume. Different sample preparation procedures were evaluated such as dilution in water or acid and microwave-assisted decomposition using concentrated or diluted acids. The optimized flow system was applied to determine Ca in eleven commercial milk samples and two standard reference materials diluted in water. Similar calcium levels were encountered comparing the results obtained by the proposed method (dilution in water) with those obtained using microwave-oven digestion. Results obtained in two standard reference materials were in agreement at 95% confidence level with those certified. Recoveries of spiked samples were in the 93% - 116% range. Relative standard deviation (n = 12) was < 5.4% and the sample throughput was 150 measurements per hour, corresponding to a consumption of 250 µL of sample and 6.25 mg La per determination.

Resumo em Inglês:

The inhibition of the corrosion of mild steel in 2M hydrochloric acid solutions by Pyridoxol hydrochloride (PXO) has been studied using weight loss and hydrogen evolution techniques. The inhibitor (PXO) exhibited highest inhibition efficiency of 71.93% at the highest inhibitor concentration of 1.0 x 10-2M investigated and a temperature of 303K from weight loss result. Also, inhibition was found to increase with increasing concentration of the inhibitor and decreasing temperature. A first order type of mechanism has been deduced from the kinetic treatment of the weight loss results and the process of inhibition attributed to physical adsorption. The results obtained from the two techniques show that pyridoxol hydrochloride could serve as an effective inhibitor of the corrosion of mild steel in HCl acid solution. The compound obeys the Langmuir adsorption isotherm equation.

Resumo em Português:

Copolímeros de metacrilato de metila (MMA) e dimetacrilato de trietilenoglicol (TEGDMA) obtidos por fotopolimerização usando complexos de Fe(III) como fotoiniciador foram submetidos a analíse térmica, TG e DSC, sob atmosfera de ar e de N2. Eventos térmicos foram observados entre 90 -110 ºC. Transições vítreas foram observadas acima de 100 ºC, seguida por um pico exotérmico à 170 ºC. O pico exotérmico foi atribuído ao processo de cura térmica devido a presença de grupos vinilícos dos monômeros que não se converteram. A técnica de DSC revelou ser uma ferramenta útil para avaliar o processo de cura desse tipo de material, usando pequenas quantidades de amostras e um curto tempo de analíse.

Resumo em Inglês:

Copolymers of methyl methacrylate (MMA) and triethyleneglycol dimethacrylate (TEGDMA) obtained by photoinitiated polymerization using Fe(III) complexes were submitted to thermogravimetry (TGA) under dynamic air atmosphere and N2, and differential scanning calorimetric analysis (DSC). Thermal events were observed only between 90 - 110 ºC. Glass transitions were observed at ca. 100 ºC, followed by an exothermic peak at 170 ºC. The exothermic peak was assigned to a thermal curing process due to the presence of unreacted vinyl groups of the monomers. DSC revealed to be a useful tool to evaluate the curing completeness in this kind of material, using small amounts of sample in relatively short time.

Resumo em Português:

O propósito deste trabalho foi determinar os parâmetros cinéticos de decomposição térmica para uma amostra de propelente base simples e base dupla. Os dados obtidos pela calorimetria exploratória diferencial foram ajustados para o modelo cinético de pseudo-primeira ordem de Flynn, Wall e Ozawa. Os respectivos parâmetros obtidos foram: BS REX 1200 (Ea) (2,3 ± 0,2) 10² kJ mol-1 e (A) 1,34 10(25) min-1; BD-111 (Ea) (1,6 ± 0,1) 10² kJ mol-1 e (A) 3,31 10(17) min-1. O espectro de infravermelho da amostra de propelente base dupla indicou a presença de salicilato, justificando o comportamento de decomposição observado na respectiva curva térmica.

Resumo em Inglês:

The purpose of this work was to determine the kinetics parameters of the thermal decomposition of a sample single-base (BS) and double-base (BD) propellants. The experimental data obtained by differential scanning calorimetry (DSC) were adjusted to the pseudo-first order kinetic model of Flynn, Wall and Ozawa. The respective parameters obtained are: BS REX 1200 (Ea) (2.3 ± 0.2) 10² kJ mol-1 and (A) 1.34 10(25) min-1; BD-111 (Ea) (1.6 ± 0.1) 10² kJ mol-1 and (A) 3.31 10(17) min-1. IR spectrum has confirmed the presence of salicilate in the double-base (BD) propellant and some correlations corroborate the conclusions about the decomposition mechanism.

Resumo em Português:

Amostra de esmectita pertencente a Serra de Maicuru (Estado do Pará, Norte do Brasil, região amazônica) foi pilarizada com Al13, A Argila pilarizada com alumínio (Al-PILC) foi caracterizada por DRX, MEV e EDS. Para a análise textural foram utilizadas isotermas de adsorção-desorção utilizando o nitrogênio. Este artigo é dirigido ao estudo da adsorção de metais pesados. A adsorção dos íons de Cu2+, Ni2+e Co2+ foi realizadas com a matriz Al-PILC em temperatura ambiente com soluções aquosas contendo os íons metálicos. Os modelos de adsorção adotados foram os de Langmuir, Freundlich e Temkin que foram aplicados aos valores obtidos experimentalmente com regressão linear. A equação de Langmuir foi o melhor modelo de linearização com r = 0,999. A equação de Freundlich apresentou limitações em altas concentrações, mas foram obtidos valores (Kf e n) bastante aceitáveis utilizando este modelo. Os parâmetros foram utilizados para calcular a quantidade de Nf em função de Cs.

Resumo em Inglês:

Smectite sample from the Serra de Maicuru area (Pará state, northern Brazil, Amazon region) were used for the pillaring process with Al13. Aluminum pillared clay (Al-PILC) was characterized by XRD, SEM and EDS. the textural analysis using nitrogen adsorption-desorption isotherms. The aim of this paper is to study in how Al-PILC adsorb heavy metals. The adsorption of Cu2+, Ni2+, Co2+ ions from aqueous solution in room temperature by Al-PILC have been carried out. The Langmuir, Freundlich and Temkin adsorption isotherm models have been applied to fit the experimental data, with the first model well adjusted with r = 0.999. The one-surface Langmuir equation provided the best fit to the data. The Freundlich equation presented limitations in rises concentrations, but acceptable values of parameters were obtained (Kf and n) with the use of the three models. The parameters were used to calculate the amount adsorbed Nf, a function constant Cs.

Resumo em Inglês:

Zorflex® activated carbon fibers (ACF), reference FM100 198B, are used before and after an oxidizing procedure with H3PO4 to study the adsorption of Pb2+. The point of zero charge was determined for the modified and unmodified fiber giving values of 2.3 and 4.3, respectively. After oxidizing the ACF, the fiber showed to have a greater Pb2+ adsorption capacity in comparison with the unmodified fiber, which is related with the acid sites increase, where lead was mainly adsorbed. Determination of the BET area was carried out by nitrogen physisorption at 77K. ACFs presented superficial areas between 1000 and 1500 m²/g showing mostly, a microporous structure. The preliminary design of an adsorbent using the modified fiber is presented where the fiber superior physicochemical properties over the unmodified one are observed.

Resumo em Inglês:

Electrode kinetics and study of 'transition state' with applied potential in case of [M - antibiotics - cephalothin] system were reported at pH = 7.30 ± 0.01 at suitable supporting electrolyte at 25.0ºC. The M = Co or Ni and antibiotics were doxycycline, chlortetracycline, oxytetracycline, tetracycline, minocycline, amoxicillin and chloramphenicol used as primary ligands and cephalothin as secondary ligand. Kinetic parameters viz. transfer coefficient (a), degree of irreversibility (l), diffusion coefficient (D) and rate constant (k) were determined. The values of a and k varied from 0.41 to 0.59 and 2.60 X 10-3 cm s-1 to 9.67 X 10-3 cm s-1 in case of [Co - antibiotics - cephalothin] system. In case of [Ni - antibiotics - cephalothin], a and k varied from 0.41 to 0.58 and 2.34 X 10-3 cm s-1 to 9.19 X 10-3 cm s-1 respectively confirmed that transition state behaves between oxidant and reductant response to applied potential and it adjusts it self in such a way that the same is located midway between dropping mercury electrode and solution interface. The values of rate constant confirmed the quasireversible nature of electrode processes. The stability constants (logb) of complexes were also determined.